EP1701798B1 - Spritzvorrichtung und verfahren zur wirbelschichtgranulation - Google Patents

Spritzvorrichtung und verfahren zur wirbelschichtgranulation Download PDF

Info

Publication number
EP1701798B1
EP1701798B1 EP03783002A EP03783002A EP1701798B1 EP 1701798 B1 EP1701798 B1 EP 1701798B1 EP 03783002 A EP03783002 A EP 03783002A EP 03783002 A EP03783002 A EP 03783002A EP 1701798 B1 EP1701798 B1 EP 1701798B1
Authority
EP
European Patent Office
Prior art keywords
gas
liquid
nozzle
spraying device
mixing chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP03783002A
Other languages
English (en)
French (fr)
Other versions
EP1701798A1 (de
Inventor
Rob Stevens
Luc Vanmarcke
Roeland Elderson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yara International ASA
Original Assignee
Yara International ASA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yara International ASA filed Critical Yara International ASA
Publication of EP1701798A1 publication Critical patent/EP1701798A1/de
Application granted granted Critical
Publication of EP1701798B1 publication Critical patent/EP1701798B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/04—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge
    • B05B7/0416—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid
    • B05B7/0441—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid with one inner conduit of liquid surrounded by an external conduit of gas upstream the mixing chamber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/06—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane
    • B05B7/062—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet
    • B05B7/066—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet with an inner liquid outlet surrounded by at least one annular gas outlet

Definitions

  • the invention concerns a spraying device for use in high capacity fluid bed granulation and a method for preparation of solid granules from a liquid material in a fluid bed.
  • this invention relates to spray nozzles usable for supplying granule-growth liquid, by atomising the liquid in a fluidised bed of solid particles where upon the microscopic liquid drops are sprayed.
  • the HFT granulation process combines very high capacity with excellent product properties and low energy consumption. In achieving this, the way of spraying the liquid to be granulated into the fluidised bed is of the highest importance.
  • the design of the nozzles where the liquid is atomised influence the liquid flow capacity - and thus the capacity of the granulator - as well as the pressure and volume flow of atomisation gas required to maintain spouts with continuous and uniform sprays without agglomeration and unwanted disturbance of the fluidised bed. Finally the nozzle design also influences the energy consumption of the granulator through its flow and pressure characteristics.
  • nozzles are generally of the binary type atomising nozzles, where a gas, e.g. air, is used to atomise the liquid to be granulated.
  • a gas e.g. air
  • the gas and liquid may be introduced through the nozzle in the same single tube, or gas and liquid may be introduced separately through for example concentric tubes so that the mixing takes place only in and after the nozzle aperture.
  • the principle aims are effective gas-liquid mixing; uniform and small size of liquid particles and a suitable geometry of the resulting spray or spout, so that the atomised liquid (microscopic droplets) are continuously and homogenously accreted on the granules formed in the fluidised bed.
  • Nozzles for use in a granulation process is for example described in generic US patent No. 4 701 353 . These have a central channel through which the liquid material is supplied, and a channel concentric therewith carrying a powerful gas stream. The liquid is passed through a rotation chamber before it is mixed with the gas stream. The nozzle may also have a concentric outer channel for providing a less energy-rich gas stream.
  • this nozzle design has limitations in liquid flow capacity and in the energy required for both nebulising or atomising the liquid into suitable droplets and at the same time fluidising the droplets into a properly shaped spout where the particle growth will occur.
  • the rotation chamber described by US 4701353 will only serve to give the liquid a helical movement, while the mixing chamber of the novel device described below will allow a thorough mixing of atomising gas and liquid before the spray leaves the exit aperture of the nozzle. Thereby the kinetic energy from the gas and liquid is utilised optimally.
  • the novel device and method described herein demonstrate high granulation capacity and low energy consumption; several times better than the values quoted in US patent No. 4 701 353 .
  • the object of the invention is to obtain a granulation process with reduced energy consumption and enhanced granulation capacity; both factors reducing the variable costs of the granulation step. Another object is to obtain granules of better quality.
  • the invention thus concerns a spraying device for melt granulation in fluidised bed comprising a nozzle with a feed channel for a liquid to be atomised, where the liquid is led through emulsifying means and into an internal mixing chamber for gas and liquid, before it is fed to the fluidised bed.
  • the nozzle has a separate channel for the atomising gas fitted concentrically around the central liquid supply channel for the liquid to be atomised or nebulised.
  • the mixing chamber surrounds the outlet zone of the liquid spray from the emulsifying means and the gas, allowing efficient mixing of high speed atomisation gas and liquid, and having an external gas cap where fluidisation gas is channelled into a spout above the spraying device.
  • the gas cap is conical and fitted to a perforated bottom plate, concentrically around the nozzle.
  • the mixing chamber could be cylindrical with an upper conical part or conical.
  • the length/diameter ratio UD of the mixing chamber should be within the range 0.5 to 5 and the I/d ratios in the range 0.1 to 2.
  • the ratio L/D of the mixing chamber is in the range 1 to 4 and the I/d ratios in the range 0.25 to 1.
  • the gas cap should have a height of 10 to 200 mm above the bottom plate (3), preferably 20 to 100 mm.
  • the upper aperture diameter of the gas cap is 20 to 150 mm and the bottom aperture diameter of 30 to 300 mm, preferably 35 to 100 mm and 40 to 200 mm, respectively.
  • the invention also concerns a method for preparation of solid granules in a fluidised bed, where a liquid material is atomised by supply of an atomising gas and sprayed into the fluidised bed through spray nozzles mounted vertically and where the fluidised bed is maintained by fluidisation gas blown upwards through a perforated plate underneath the bed.
  • a portion of the fluidisation gas should be channelled through a gas cap surrounding the nozzle for creation of a gas spout above the spraying device.
  • the invention also concerns a method for preparation of solid granules from a liquid material in a fluidised bed by using a nozzle with a feed channel for a liquid to be atomised.
  • the liquid is led through emulsifying means and into an internal mixing chamber for gas and liquid, before spraying the atomised liquid upwardly into the fluid bed layer.
  • the atomising gas is led through a channel concentrically to the liquid supply and into the mixing chamber surrounding the outlet openings for both liquid and gas, allowing efficient mixing of high speed atomisation gas and liquid.
  • a portion of the fluidisation gas is channelled through a gas cap surrounding the nozzle for creating a gas spout above the spraying device.
  • the spraying device could be used for production of granules of urea, and other fertiliser products, such as calcium ammonium nitrate, ammonium nitrate, ammonium sulphate and mixtures thereof.
  • the liquid is sprayed into a fluidised bed through spray nozzles mounted vertically and spraying the atomised liquid upwardly into the fluid bed layer.
  • the fluidised layer is maintained by fluidisation gas blown upwards through a perforated plate underneath the bed.
  • the nozzles are placed in openings in this plate with their apertures a given distance. e.g. 5 - 100 mm, above the plate.
  • the design of the nozzles where the liquid is atomised influences the liquid flow capacity and thus the capacity of the granulator. It also influences the pressure and volume rate of atomisation gas required to maintain spouts with continuous and uniform sprays, without unwanted agglomeration and disturbance of the fluidised bed. Finally the nozzle design also influences the energy consumption of the granulator through its gas flow characteristics. This has a direct impact on the variable costs of the operation.
  • the nozzle should atomise the liquid into droplets at desired size, approximately 50-100 micron for a single phase melt. At the same time the nozzle should evaporate some of the water, without creating premature solidification. It should also distribute and deliver droplets into the bed at the same time as it should contribute to movement around the nozzle and mass exchange in the bed.
  • the main novelty of the invention is the use of low energy fluidisation gas to replace a large portion of the high-pressure atomisation gas required. This is achieved by channelling the fluidisation gas through a specially designed gas cap surrounding the nozzle, thus creating a gas spout. A novel mixing chamber upstream from the nozzle aperture improves the internal mixing of gas and liquid in the atomisation process in the nozzle.
  • the present invention has effected that the granule quality characteristics and granulation capacity may be maintained or even improved, while energy consumption is considerably reduced, compared to those nozzles hitherto used in granulation.
  • the reduced energy consumption is obtained because the atomisation gas can be operated at lower pressure, without increasing the total amount of fluidisation gas. This design still allows a high melt throughput and excellent physical characteristics of the granules.
  • Figure 2A the design of the gas cap and position of gas cap concentrically outside the nozzle is shown.
  • Figure 2B shows a horizontal section along A-A.
  • the conically shaped gas cap 1 is mounted concentrically around the nozzle 2 on a perforated sieve plate 3 and exposed to fluidisation gas.
  • the top diameter of the gas cap device is smaller than the bottom diameter, and there is clearance for gas passage between the outer nozzle wall and the gas cap.
  • the amount of gas through the gas cap shall be sufficient to create a viable spout into the granulator bed.
  • the velocity of gas through the gas cap is determined by the horizontal area between nozzle and gas cap, the upper diameter of the gas cap aperture and the diameter of the bottom inlet of the gas cap.
  • the mass flow of fluidisation gas per square meter horizontal bed area remains almost unchanged from the known designs.
  • Figure 3 shows the new nozzle design with cylindrical mixing chamber.
  • the ratio length: diameter (UD) of the mixing chamber could be varied as indicated in the drawing.
  • Omitted from the figure are feed lines, the perforated bottom plate of the granulator and the conical cap mounted concentrically to the nozzle on the bottom plate.
  • the nozzle 2 is composed of a central channel 4 which at one end A connects with a liquid line omitted from the drawing and at the other end leads B into a mixing chamber 5.
  • a swirling device 6 is mounted inside to bring the feed via A in helical motion at point B.
  • the spraying device is provided with a channel 7 which has been fitted concentrically around the central liquid supplying channel 4.
  • Channel 7 being at one end connected to a gas line omitted from the drawing and at the other end provided with 5-15 round holes 8, which leads into the mixing chamber 5.
  • the two continuous flows are fed inside the mixing chamber at the same time: a granule's growth liquid through opening B and a gas flow via 8.
  • a gas in liquid emulsion can be generated.
  • Expansion through the orifice opening 9 converts the emulsion to droplets of 50 - 100 ⁇ m diameter, which are suitable for granule growth in the fluidised bed.
  • Figure 4 shows a nozzle with a conical mixing chamber 5. The other parts of the nozzle are the same as in Figure 3 .
  • the UD ratio should be in the range 0.5 to 5, and the I/d ratio in the range 0.1 to 2 in order to efficiently obtain droplets with average diameter less then 100 ⁇ m.
  • UD should range from 1 to 4 and I/d from 0.25 to 1.
  • the invention will be further illustrated by the following examples describing granulation of urea.
  • the examples will demonstrate values obtained for product quality parameters as well as energy consumptions for a range of nozzles based on the novel design.
  • a granulator was fit with the experimental nozzle in the centre.
  • the conical gas cap had a lower diameter of 105 mm and an upper diameter of 50 mm. It was mounted on a 4.5% opening perforated sieve plate containing holes of 2 mm in diameter.
  • the amount of air through this gas cap was 248 Nm 3 /h under a feed pressure equal to the fluidisation gas (air) pressure of about 800 mmwc and with a temperature of 40 °C.
  • the granulations were carried out under normal standard urea granulation conditions with a melt of 96% urea containing 0.55 wt.% formaldehyde, with a temperature of about 132 °C.
  • the set-up was supplied with fluidisation gas necessary to keep the bed in movement and also for creating a spout via the gas cap 'spout opening'.
  • the atomisation gas with a flow rate of 32 kg/h and a temperature of 142 °C was supplied together with the melt into the nozzle's mixing chamber.
  • Product quality parameters such as moisture content, density, crushing strength of the granules with diameter 2.5-4.5 mm were analysed for each nozzle test. During the test different liquid flows have been used; 250, 350 and 450 I/h. Each granulation test was at least carried out in duplicate.
  • Example 3 Nozzle with conical mixing chamber
  • This mixing chamber nozzle with conical shape has also 12 inlet gas openings (D), which are placed, in an angle directed towards the rotational direction of the liquid swirl. It is constructed to give the atomisation gas a rotation in opposite direction to the liquid, in order to make a maximum impact of gas into the liquid flow.
  • Table 6 Operating parameters Nozzle : HFT design Novel design Conical (prior art) Ex. A Ex. B Urea feed flow kg/h 540 450 375 Urea feed pressure bar 1.4 1.4 1.9 Fluid. gas (air) flow kg/m 2 .h 7952 7952 8107 Fluid. gas (air) pressure mmwc 800 800 800 bar 0.08 0.08 0.08 Spout. gas (air) flow kg/h - - 320 Atom.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Fertilizers (AREA)
  • Glanulating (AREA)
  • Nozzles (AREA)
  • Dairy Products (AREA)

Claims (9)

  1. Sprühvorrichtung zur Schmelzgranulation in einem Wirbelbett, umfassend eine Düse (2) mit einem Zuführungskanal (4) für eine zu zerstäubende Flüssigkeit, wo die Flüssigkeit durch eine Emulgiereinrichtung (6) und in eine innere Mischkammer (8) für Gas und Flüssigkeit geführt wird, bevor sie dem Wirbelbett zugeführt wird, wobei die Düse (2) einen separaten Kanal (7) für das Zerstäubergas aufweist, der konzentrisch um den zentralen Flüssigkeits-Zuführungskanal (4) für die zu zerstäubende oder zu vernebelnde Flüssigkeit gepasst ist, und wo die Mischkammer (5) die Auslasszone des Flüssigkeitssprühnebels aus der Emulgiereinrichtung und das Gas umgibt, wobei ein effizientes Mischen des Hochgeschwindigkeits-Zerstäubergases und der Flüssigkeit zugelassen wird, und eine äußere Gaskappe (1) aufweist, wo Fluidisierungsgas in einen Ausfluss über der Sprühvorrichtung kanalisiert wird, dadurch gekennzeichnet, dass die Gaskappe (1) konisch und an eine perforierte Bodenplatte (3) gepasst ist, konzentrisch um die Düse (2) herum.
  2. Sprühvorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass die Mischkammer (5) zylindrisch mit einem oberen konischen Teil ist.
  3. Sprühvorrichtung nach Anspruch 1 oder Anspruch 2, dadurch gekennzeichnet, dass das Verhältnis zwischen der Länge (L) und dem Durchmesser (D) der Mischkammer (5) in dem Bereich von 0,5 bis 5 liegt, vorzugsweise 1 bis 4, und die Länge (1) und der Durchmesser (d) der Öffnung (9) in dem Bereich von 0,1 bis 2 liegt, vorzugsweise 0,25 bis 1.
  4. Sprühvorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass die Mischkammer (5) konisch ist.
  5. Sprühvorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Gaskappe (1) eine Höhe von 10 bis 200 mm über der Bodenplatte (3) aufweist, vorzugsweise 20 bis 100 mm.
  6. Sprühvorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Gaskappe (1) einen oberen Durchlassdurchmesser von 20 bis 150 mm aufweist und einen unteren Durchlassdurchmesser von 30 bis 300 mm, vorzugsweise 35 bis 100 mm beziehungsweise 40 bis 200 mm.
  7. Verfahren zur Zubereitung von Festkörper-Granulat in einem Wirbelbett, wo ein flüssiges Material durch Zuführung eines Zerstäubergases zerstäubt und in das Wirbelbett durch Sprühdüsen (2) gesprüht wird, die vertikal montiert sind, und wo das Wirbelbett durch ein Fluidisierungsgas beibehalten wird, das nach oben durch eine perforierte Platte unterhalb des Bettes geblasen wird, dadurch gekennzeichnet, dass ein Teil des Fluidisierungsgases durch eine Gaskappe (1) kanalisiert wird, die die Düse umgibt, zur Bildung eines Gasausflusses über der Sprühvorrichtung.
  8. Verfahren zur Zubereitung von Festkörper-Granulat aus einem flüssigen Material in einem Wirbelbett durch Verwendung einer Düse (2) mit einem Zuführungskanal (4) für eine zu zerstäubende Flüssigkeit, wo die Flüssigkeit durch eine Emulgiereinrichtung und in eine innere Mischkammer (5) für Gas und Flüssigkeit geführt wird, bevor die zerstäubte Flüssigkeit nach oben in die Wirbelbettschicht gesprüht wird, dadurch gekennzeichnet, dass das Zerstäubergas zu der Mischkammer (5) in einem Kanal (7), konzentrisch zu der Flüssigkeit, und in die Mischkammer geführt wird, die Ablassdurchtrittsöffnungen für beide, die Flüssigkeit und das Gas, umgibt, wobei ein effizientes Mischen des Hochgeschwindigkeits-Zerstäubergases und der Flüssigkeit zugelassen wird, und wo ein Teil des Fluidisierungsgases durch eine Gaskappe (1) kanalisiert wird, die die Düse (2) umgibt, womit ein Gasausfluss über der Sprühvorrichtung gebildet wird.
  9. Verwendung einer Sprühvorrichtung nach einem der Ansprüche 1 bis 6 in einem Verfahren zur Zubereitung von granulatförmigem Urea und anderen Schmelzen, die zum Produzieren von Düngemittelprodukten geeignet sind, wie beispielsweise Calciumammoniumnitrat, Ammoniumnitrat, Ammoniumsulfat und Mischungen daraus.
EP03783002A 2003-12-23 2003-12-23 Spritzvorrichtung und verfahren zur wirbelschichtgranulation Expired - Lifetime EP1701798B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/NO2003/000440 WO2005061118A1 (en) 2003-12-23 2003-12-23 Spraying device and method for fluidised bed granulation

Publications (2)

Publication Number Publication Date
EP1701798A1 EP1701798A1 (de) 2006-09-20
EP1701798B1 true EP1701798B1 (de) 2010-05-19

Family

ID=34709402

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03783002A Expired - Lifetime EP1701798B1 (de) 2003-12-23 2003-12-23 Spritzvorrichtung und verfahren zur wirbelschichtgranulation

Country Status (12)

Country Link
US (1) US7704420B2 (de)
EP (1) EP1701798B1 (de)
CN (1) CN1972754B (de)
AR (1) AR048140A1 (de)
AT (1) ATE468176T1 (de)
AU (1) AU2003290465A1 (de)
BR (1) BR0318663B1 (de)
CA (1) CA2549755C (de)
DE (1) DE60332664D1 (de)
EG (1) EG24629A (de)
ES (1) ES2346137T3 (de)
WO (1) WO2005061118A1 (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017005695A1 (en) 2015-07-07 2017-01-12 Yara International Asa Method for the manufacture of a urea-based particulate material containing elemental sulphur
EP3309137A1 (de) 2016-10-13 2018-04-18 YARA International ASA Verbesserte harnstoffbasierte zusammensetzung mit elementarem schwefel und verfahren zur herstellung davon
EP3372576A1 (de) 2017-03-07 2018-09-12 Yara International ASA Harnstoffbasierte zusammensetzung und verfahren zur herstellung davon
EP3639916A1 (de) 2018-10-18 2020-04-22 Yara International ASA Verfahren und wirbelschichtgranulator zur herstellung von granulaten aus einer aufschlämmung
WO2021028460A1 (en) 2019-08-12 2021-02-18 Yara International Asa Improved urea-based composition and method for the manufacture thereof

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7819071B2 (en) * 2006-11-16 2010-10-26 Seminatore Salvatore J Nozzle system
EP2163364B1 (de) * 2007-06-11 2012-05-16 National University Corporation Kyoto Institute of Technology Pflanzenverarbeitungsverfahren
EP2177273A1 (de) 2008-10-16 2010-04-21 Urea Casale S.A. Sprühverfahren und Düse zur Zerstäubung einer Flüssigkeit
US8225602B2 (en) * 2009-06-11 2012-07-24 Stanadyne Corporation Integrated pump and injector for exhaust after treatment
US20100314470A1 (en) * 2009-06-11 2010-12-16 Stanadyne Corporation Injector having swirl structure downstream of valve seat
JP5471675B2 (ja) * 2010-03-23 2014-04-16 アイシン精機株式会社 オイル圧制御装置
US8794744B2 (en) * 2011-09-14 2014-08-05 Shenzhen China Star Optoelectronics Technology Co., Ltd. Inkjet unit and inkjet device
JP6166103B2 (ja) * 2013-06-04 2017-07-19 ヤンマー株式会社 尿素水噴射ノズル
CN103363519A (zh) * 2013-08-05 2013-10-23 瓮福（集团）有限责任公司 一种沸腾炉风帽
CN105579566B (zh) 2013-08-28 2020-01-10 索理思科技公司 谷物加工中的采油助剂
CN103657894B (zh) * 2013-12-06 2017-04-19 北京京能电力股份有限公司石景山热电厂 用于尿素热解制氨工艺的溶液雾化装置
ES2788743T3 (es) * 2014-10-09 2020-10-22 Spraying Systems Mfg Europe Gmbh Boquilla de atomización
DE102015006727A1 (de) * 2015-05-30 2016-12-01 Rainer Pommersheim Verfahren und technischer Prozess zur Herstellung von Mikro- und Nanopartikeln unterschiedlicher Größe
CN107838429B (zh) * 2017-10-17 2021-06-04 广西金川有色金属有限公司 一种高效率的高温熔体粒化装置
EP3581265A1 (de) 2018-06-12 2019-12-18 thyssenkrupp Fertilizer Technology GmbH Sprühdüse zur herstellung eines harnstoff-schwefel düngers
CN109985745B (zh) * 2019-04-10 2020-07-28 业成科技（成都）有限公司 可提高曲面喷涂均匀性之喷涂装置
CN112439570A (zh) * 2020-11-10 2021-03-05 中国船舶重工集团公司第七0七研究所 一种用于微量润滑切削的静电雾化喷嘴及其使用方法

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE367121B (de) * 1972-10-13 1974-05-20 Alfa Laval Ab
US3979069A (en) * 1974-10-11 1976-09-07 Luigi Garofalo Air-atomizing fuel nozzle
FR2522991A1 (fr) * 1982-03-08 1983-09-16 G2M Lepetit Appareil de pulverisation pneumatique de liquide sous forme d'un jet
NL8302999A (nl) * 1983-08-27 1985-03-18 Unie Van Kunstmestfab Bv Werkwijze voor het bereiden van granules.
NL8303000A (nl) 1983-08-27 1985-03-18 Unie Van Kunstmestfab Bv Werkwijze voor het bereiden van granules.
US4555059A (en) * 1984-08-06 1985-11-26 Vortec Corporation Flow-amplifying liquid-atomizing nozzle
KR0159947B1 (ko) * 1991-03-12 1998-11-16 마사아키 오카와라 분수형 가압 2류체 노즐 장치와 그것을 편입하여 이루어지는 스프레이 드라이어 장치, 및 가압 2류체에 있어서의 액적 경 제어법
US5236503A (en) * 1991-10-28 1993-08-17 Glatt Air Techniques, Inc. Fluidized bed with spray nozzle shielding
RU2104258C1 (ru) * 1992-08-07 1998-02-10 Хидро Агри Слейскил Б.В. Способ производства гранул мочевины
JP3929000B2 (ja) 1998-05-08 2007-06-13 アイセロ化学株式会社 高純度薬品液用容器
AU765160B2 (en) * 1998-12-18 2003-09-11 Symrise Gmbh & Co. Kg Encapsulated flavour and/or fragrance preparations
CA2375406C (en) * 1999-06-21 2005-10-18 The Procter & Gamble Company Processes for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017005695A1 (en) 2015-07-07 2017-01-12 Yara International Asa Method for the manufacture of a urea-based particulate material containing elemental sulphur
EP4101828A1 (de) 2015-07-07 2022-12-14 Yara International ASA Verfahren zur herstellung eines partikelförmigen materials auf harnstoffbasis mit elementarem schwefel
EP3309137A1 (de) 2016-10-13 2018-04-18 YARA International ASA Verbesserte harnstoffbasierte zusammensetzung mit elementarem schwefel und verfahren zur herstellung davon
WO2018069486A2 (en) 2016-10-13 2018-04-19 Yara International Asa Improved urea-based composition comprising elemental sulphur and method for the manufacture thereof
EP3372576A1 (de) 2017-03-07 2018-09-12 Yara International ASA Harnstoffbasierte zusammensetzung und verfahren zur herstellung davon
WO2018162533A1 (en) 2017-03-07 2018-09-13 Yara International Asa Improved urea-based composition and method for the manufacture thereof
EP3639916A1 (de) 2018-10-18 2020-04-22 Yara International ASA Verfahren und wirbelschichtgranulator zur herstellung von granulaten aus einer aufschlämmung
WO2021028460A1 (en) 2019-08-12 2021-02-18 Yara International Asa Improved urea-based composition and method for the manufacture thereof

Also Published As

Publication number Publication date
US7704420B2 (en) 2010-04-27
EG24629A (en) 2010-03-09
CA2549755A1 (en) 2005-07-07
CA2549755C (en) 2012-05-15
AU2003290465A1 (en) 2005-07-14
BR0318663B1 (pt) 2012-01-24
EP1701798A1 (de) 2006-09-20
DE60332664D1 (de) 2010-07-01
BR0318663A (pt) 2006-11-28
CN1972754B (zh) 2010-11-03
WO2005061118A1 (en) 2005-07-07
ES2346137T3 (es) 2010-10-11
CN1972754A (zh) 2007-05-30
AR048140A1 (es) 2006-04-05
US20070200007A1 (en) 2007-08-30
ATE468176T1 (de) 2010-06-15

Similar Documents

Publication Publication Date Title
EP1701798B1 (de) Spritzvorrichtung und verfahren zur wirbelschichtgranulation
CA2245992C (en) Method for granulation and granulator
US20240042480A1 (en) Fluid Bed Granulation Process and Apparatus
AU2002338492B2 (en) Fluid bed granulation apparatus
US6159252A (en) Process and device for producing granulates by fluidized bed spray granulation
JPS6097037A (ja) グラニユ−ルの製造法
AU2002338492A1 (en) Fluid bed granulation apparatus
US7628838B2 (en) Method for producing particle-shaped material
US7344663B2 (en) Multi-nozzle for granulation and method for manufacturing granular product
JPS5910961B2 (ja) ヨウユウキンゾクオビリユウカスルホウホウ オヨビ ソウチ
WO2003000397A1 (fr) Dispositif de traitement de particules de poudre
US20030098360A1 (en) Twin fluid centrifugal nozzle for spray dryers
RU2325956C2 (ru) Распылительное устройство и способ грануляции псевдоожиженного слоя
JPH10216499A (ja) 改良された造粒方法及び造粒器
PL208979B1 (pl) Urządzenie rozpylające do granulacji roztopionego materiału w złożu fluidalnym, (54) sposób przygotowywania stałych granulek w złożu fluidalnym oraz sposób wytwarzania stałych granulek z ciekłego materiału w złożu fluidalnym

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20060721

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: LT

RAX Requested extension states of the european patent have changed

Extension state: LT

Payment date: 20060721

17Q First examination report despatched

Effective date: 20070906

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: LT

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REF Corresponds to:

Ref document number: 60332664

Country of ref document: DE

Date of ref document: 20100701

Kind code of ref document: P

REG Reference to a national code

Ref country code: RO

Ref legal event code: EPE

REG Reference to a national code

Ref country code: NL

Ref legal event code: T3

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2346137

Country of ref document: ES

Kind code of ref document: T3

LTIE Lt: invalidation of european patent or patent extension

Effective date: 20100519

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100820

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100920

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20100519

26N No opposition filed

Effective date: 20110222

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 60332664

Country of ref document: DE

Effective date: 20110221

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20101231

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20101231

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20101223

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20101231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20101223

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101120

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 13

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 14

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 15

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: RO

Payment date: 20221123

Year of fee payment: 20

Ref country code: NL

Payment date: 20221114

Year of fee payment: 20

Ref country code: GB

Payment date: 20221103

Year of fee payment: 20

Ref country code: FR

Payment date: 20221110

Year of fee payment: 20

Ref country code: DE

Payment date: 20220622

Year of fee payment: 20

Ref country code: BG

Payment date: 20221011

Year of fee payment: 20

Ref country code: AT

Payment date: 20221125

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20230110

Year of fee payment: 20

Ref country code: TR

Payment date: 20221222

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 60332664

Country of ref document: DE

REG Reference to a national code

Ref country code: NL

Ref legal event code: MK

Effective date: 20231222

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20240102

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Expiry date: 20231222

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20231222

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20231224

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20231222

Ref country code: ES

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20231224

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK07

Ref document number: 468176

Country of ref document: AT

Kind code of ref document: T

Effective date: 20231223